Ethylene Glycol → Ethyl 1,4-dioxaspiro(4.5)decane-8-carboxylate

HRID 12639

반응식

HRID 12639 반응식
[CH2:1]([O:3][C:4]([CH:6]1[CH2:11][CH2:10][C:9](=[O:12])[CH2:8][CH2:7]1)=[O:5])[CH3:2].[CH2:13](O)[CH2:14][OH:15].C1(C)C=CC(S(O)(=O)=O)=CC=1.C(OCC)C>C1(C)C=CC=CC=1>[CH2:1]([O:3][C:4]([CH:6]1[CH2:11][CH2:10][C:9]2([O:15][CH2:14][CH2:13][O:12]2)[CH2:8][CH2:7]1)=[O:5])[CH3:2]

참가 물질

6

반응물 4

HCID 174Ethylene GlycolHCID 3283Diethyl EtherHCID 6101p-Toluenesulfonic acidHCID 317638Ethyl 4-oxocyclohexanecarboxylate

생성물 1

HCID 10488810Ethyl 1,4-dioxaspiro(4.5)decane-8-carboxylate

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

4-oxo-cyclohexanecarboxylic acid ethyl ester (52.8 g, 0.31 mole, Merck, Order No. 814249), ethylene glycol (67.4 g, 1.08 mole) and p-toluenesulfonic acid (0.7 g) in toluene (160 ml) were stirred for 20 hours at RT, and the reaction solution was poured into diethyl ether (300 ml) and washed with water, sodium hydrogen carbonate solution and sodium chloride solution. The solution was dried (Na2SO4), concentrated by evaporation in vacuo, and the remaining colorless liquid was processed further without purification.

후처리

  1. washwashed with water, sodium hydrogen carbonate solution and sodium chloride solution
  2. dry with materialThe solution was dried (Na2SO4)
  3. concentrationconcentrated by evaporation in vacuo
  4. customthe remaining colorless liquid was processed further without purification

출처 및 근거

ORD 기록
ord-cf51c88887784dd4a140c68d1eeaed7a
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728028B2

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